CN105271237A - Induction plasma preparation method of single-specification nano silicon powder - Google Patents
Induction plasma preparation method of single-specification nano silicon powder Download PDFInfo
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- CN105271237A CN105271237A CN201510683284.3A CN201510683284A CN105271237A CN 105271237 A CN105271237 A CN 105271237A CN 201510683284 A CN201510683284 A CN 201510683284A CN 105271237 A CN105271237 A CN 105271237A
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- China
- Prior art keywords
- preparation
- induction plasma
- silicon powder
- airflow milling
- silica flour
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- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 230000006698 induction Effects 0.000 title claims abstract description 21
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title abstract description 8
- 239000005543 nano-size silicon particle Substances 0.000 title abstract 4
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000012216 screening Methods 0.000 claims abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 42
- 238000000034 method Methods 0.000 claims description 33
- 229910021487 silica fume Inorganic materials 0.000 claims description 22
- 239000000377 silicon dioxide Substances 0.000 claims description 21
- 235000013312 flour Nutrition 0.000 claims description 20
- 238000003801 milling Methods 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 10
- 229920005591 polysilicon Polymers 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 239000000112 cooling gas Substances 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 238000012545 processing Methods 0.000 abstract description 22
- 239000002994 raw material Substances 0.000 abstract description 10
- 239000002245 particle Substances 0.000 abstract description 7
- 238000009826 distribution Methods 0.000 abstract description 4
- 239000011863 silicon-based powder Substances 0.000 abstract description 4
- 238000010902 jet-milling Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract 1
- 230000009466 transformation Effects 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000013467 fragmentation Methods 0.000 description 2
- 238000006062 fragmentation reaction Methods 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 238000013475 authorization Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 238000007750 plasma spraying Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 229960001866 silicon dioxide Drugs 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
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- Silicon Compounds (AREA)
Abstract
An induction plasma preparation method of single-specification nano silicon powder is characterized by comprising following steps: polycrystalline silicon powder is placed in a vacuum oven for water removal, the dried polycrystalline silicon powder is subjected to crushing, screening and airflow classification processing by the aid of a jet milling and then is subjected to induction plasma preparation, and the single-specification nano silicon powder can be obtained. Compared with the prior art, the preparation method has the advantages as follows: the preparation efficiency is higher than 300 g/h, the utilization rate of raw materials is higher than 50%, and meanwhile, the single-specification high-quality nano silicon powder with consistent structure and uniform particle size distribution can be obtained through drying, crushing, classification as well as induction plasma preparation.
Description
Technical field
The present invention relates to a kind of preparation method of nano silica fume.
Background technology
Nano silica fume is widely used in photovoltaic industry, photoelectric functional material, battery electrode material, thermoelectric material and luminescent device, nano-device, to its nano-micro structure, there is harsh requirement, reduce and even eliminate nano twin crystal, the nano crystal preparing unified structure could ensure that it has identical use properties to greatest extent.
Conventional nano silica flour, it is the chemical Vapor deposition process of raw material and fluidized bed process that preparation method mainly contains with silane, take silicon-dioxide as the redox reaction method of raw material, take polysilicon as the arc plasma method of raw material and fall method and the Siemens Method that is raw material with silicon tetrachloride and derivative thereof.Specifically can REFERENCE TO RELATED people in interim " solar level nano silica fume technology of preparing and the general situation of development " delivered of in January, 2015 the 38th volume the 1st in " Arms Material scientific and engineering ".
Nano-powder particle size distribution is wide in range, regularly there is twinning, powder use properties is caused to decline, simultaneously due to the raw material polysilicon powder footpath skewness of market purchasing, out-of-shape and surface adsorption moisture, reunite fairly obvious, flowing property is poor, powder feeding rate is unstable, easily causes powder feeding pipes to block.The too low then preparation efficiency of powder feeding rate is not high, and the gasification of powder feeding rate too high then raw material silica flour is insufficient, does not even gasify namely through plasma area, causes nanometer insufficient.Therefore, the nano silica fume how basis prepared by scale obtaining identical, the single specification of structure is the Key technique problem preparing nano silica fume.
Take polysilicon as the arc plasma method of raw material, in preparation process, electrode fouling, can introduce impurity element in the starting the arc stage, thus reduce nano silica fume purity, method of falling due to preparation technology's cycle longer, production efficiency is low, relative production cost is higher, therefore, needs to improve.
For this reason, many effort have been done in prior art, see that the patent No. is the Chinese invention patent " production method of nano silica fume " (Authorization Notice No. is CN102910630B) of ZL201210388785.5, which disclosing with silica flour is the plasma spraying process of raw material.
Summary of the invention
Technical problem to be solved by this invention is the induction plasma preparation method providing a kind of single specification nano silica fume for the above-mentioned state of the art in addition.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of induction plasma preparation method of single specification nano silica fume, it is characterized in that comprising the steps: polycrystalline silica flour, put into vacuum drying oven and remove moisture, then the polycrystalline silica flour of oven dry is carried out break process by airflow milling, screening, air classification process, then the nano silica fume that can obtain single specification through induction plasma preparation.
As preferably, described polycrystalline silica flour purity is >99.99%, and described polysilicon powder footpath is 2-40 μm.
As preferably, described baking oven vacuum tightness 10
-1-10
-3mPa, bake out temperature 70-100 DEG C, drying time 24-72h.
As preferably, described airflow milling adopts Nai Chi company model to be the airflow milling of DGS10, and the treatment condition of this airflow milling are as follows: grading wheel rotating speed 2000-16000min
-1, bearing gas 0.1-0.5bar, gap gas 0.1-0.5bar, grinding gas 4-8bar, rotating speed dosage 1%-40%, scrap rates 1-10kg/h.
As preferably, described screening adopts 200-500 eye mesh screen to sieve.
As preferably, described induction plasma preparation adopt Canadian Tyke to receive model that company produces is TIU-60 induction plasma ultrafine powder preparation apparatus, treatment condition are as follows:
Powder feeding rate 400-600g/h;
Plasma power 60kW;
Intermediate gas flow 1-1.5 standard liter/second;
Cooling gas flow 1.0-1.5 standard liter/second argon gas;
Cooling gas flow 0.5-0.8 standard liter/second hydrogen;
Chamber pressure 100kPa;
Current-carrying airshed 0.2 standard liter/second.
Compared with prior art, the invention has the advantages that: adopt high-purity polycrystalline silicon powder, uniform particle sizes, good dispersity, soilless sticking phenomenon, improves the preparation efficiency of nano silica fume and the transformation efficiency of polycrystalline silica flour effectively, preparation efficiency reaches more than 300g/h, utilization rate of raw materials reaches more than 50%, simultaneously by the process such as ovens dry, fragmentation, classification, prepares can obtain structure unanimously and the high quality nano silica fume of even particle size distribution, single specification through induction plasma.
Accompanying drawing explanation
Fig. 1 be in embodiment 1 size distribution at the electron photomicrograph of the high-purity polycrystalline silicon powder of 2-40 μm.
Fig. 2 is the electron photomicrograph of polycrystalline silica flour after drying, fragmentation, screening, classification in embodiment 1.
Fig. 3 is the electron photomicrograph of the nano silica fume of preparation in embodiment 1.
Embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
Embodiment 1, shown in composition graphs 1, Fig. 2 and Fig. 3, be that vacuum drying oven put into by high purity (>99.99%) the polycrystalline silica flour of 2-40 μm by particle diameter, processing parameter is: vacuum tightness is 10
-3mPa, bake out temperature is 100 DEG C, and drying time is 24h, and the polycrystalline silica flour of oven dry is carried out break process by resistance to (Netzsch) the airflow milling DGS10 that speeds, and processing parameter is as shown in table 2.
Table 2 airflow milling break process processing parameter
Adopt 325 eye mesh screens to sieve the polycrystalline silica flour through break process, then carry out air classification process by air classifier, processing parameter is as shown in table 3.
Table 3 air classification processing parameter
Adopt induction plasma equipment to carry out nanometer process subsequently, processing parameter is as shown in table 4.
Table 4 nanometered disposal processing parameter
After induction plasma process, the transformation efficiency of nano silica fume is as shown in table 5.
Table 5 nano silica fume transformation efficiency
Embodiment 2, be that vacuum drying oven put into by high purity (>99.99%) the polycrystalline silica flour of 2-40 μm by particle diameter, processing parameter is: vacuum tightness is 10
-2mPa, bake out temperature is 80 DEG C, and drying time is 48h, and the polycrystalline silica flour of oven dry is carried out break process by resistance to (Netzsch) the airflow milling DGS10 that speeds, and processing parameter is as shown in table 6.
Table 6 airflow milling break process processing parameter
Adopt 500 eye mesh screens to sieve the polycrystalline silica flour through break process, then carry out air classification process by air classifier, processing parameter is as shown in table 7.
Table 7 air classification processing parameter
Adopt induction plasma equipment to carry out nanometer process subsequently, processing parameter is as shown in table 8.
Table 8 nanometered disposal processing parameter
After induction plasma process, the transformation efficiency of nano silica fume is as shown in table 9.
Table 9 nano silica fume transformation efficiency
Embodiment 3, be that vacuum drying oven put into by high purity (>99.99%) the polycrystalline silica flour of 2-40 μm by particle diameter, processing parameter is: vacuum tightness is 10
-1mPa, bake out temperature is 70 DEG C, and drying time is 72h, and the polycrystalline silica flour of oven dry is carried out break process by resistance to (Netzsch) the airflow milling DGS10 that speeds, and processing parameter is as shown in table 10.
Table 10 airflow milling break process processing parameter
Adopt 200 eye mesh screens to sieve the polycrystalline silica flour through break process, then carry out air classification process by air classifier, processing parameter is as shown in table 11.
Table 11 air classification processing parameter
Adopt induction plasma equipment to carry out nanometer process subsequently, processing parameter is as shown in table 12.
Table 12 nanometered disposal processing parameter
After induction plasma process, the transformation efficiency of nano silica fume is as shown in table 13.
Table 13 nano silica fume transformation efficiency
Claims (6)
1. the induction plasma preparation method of a single specification nano silica fume, it is characterized in that comprising the steps: polycrystalline silica flour, put into vacuum drying oven and remove moisture, then the polycrystalline silica flour of oven dry is carried out break process by airflow milling, screening, air classification process, then the nano silica fume that can obtain single specification through induction plasma preparation.
2. preparation method according to claim 1, it is characterized in that described polycrystalline silica flour purity is >99.99%, described polysilicon powder footpath is 2-40 μm.
3. preparation method according to claim 1, is characterized in that described baking oven vacuum tightness 10
-1-10
-3mPa, bake out temperature 70-100 DEG C, drying time 24-72h.
4. preparation method according to claim 1, it is characterized in that described airflow milling adopts Nai Chi company model to be the airflow milling of DGS10, the treatment condition of this airflow milling are as follows: grading wheel rotating speed 2000-16000min
-1, bearing gas 0.1-0.5bar, gap gas 0.1-0.5bar, grinding gas 4-8bar, rotating speed dosage 1%-40%, scrap rates 1-10kg/h.
5. preparation method according to claim 1, is characterized in that described screening adopts 200-500 eye mesh screen to sieve.
6. preparation method according to claim 1, the model that it is characterized in that the preparation of described induction plasma adopting Canadian Tyke to receive company produces is TIU-60 induction plasma ultrafine powder preparation apparatus, and treatment condition are as follows:
Powder feeding rate 400-600g/h;
Plasma power 60kW;
Intermediate gas flow 1-1.5 standard liter/second;
Cooling gas flow 1.0-1.5 standard liter/second argon gas;
Cooling gas flow 0.5-0.8 standard liter/second hydrogen;
Chamber pressure 100kPa;
Current-carrying airshed 0.2 standard liter/second.
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| CN201510683284.3A CN105271237A (en) | 2015-10-20 | 2015-10-20 | Induction plasma preparation method of single-specification nano silicon powder |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1874838A (en) * | 2003-08-28 | 2006-12-06 | 泰克纳等离子系统公司 | Synthesis, separation and purification methods of powder materials |
| CN101439403A (en) * | 2008-12-25 | 2009-05-27 | 中国兵器工业第五二研究所 | Earlier stage treatment process of raw material powder for preparing induction plasma capacitor level nano tantalum powder |
| CN102554242A (en) * | 2012-02-09 | 2012-07-11 | 西安宝德粉末冶金有限责任公司 | Method for manufacturing micro-fine spherical titanium powder |
| WO2012148034A1 (en) * | 2011-04-26 | 2012-11-01 | 주식회사 네오플랜트 | Production method for nano silicon carbide using a thermal plasma |
| CN102910630A (en) * | 2012-10-15 | 2013-02-06 | 江苏博迁光伏材料有限公司 | Production method of nano silicon powder |
-
2015
- 2015-10-20 CN CN201510683284.3A patent/CN105271237A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1874838A (en) * | 2003-08-28 | 2006-12-06 | 泰克纳等离子系统公司 | Synthesis, separation and purification methods of powder materials |
| CN101439403A (en) * | 2008-12-25 | 2009-05-27 | 中国兵器工业第五二研究所 | Earlier stage treatment process of raw material powder for preparing induction plasma capacitor level nano tantalum powder |
| WO2012148034A1 (en) * | 2011-04-26 | 2012-11-01 | 주식회사 네오플랜트 | Production method for nano silicon carbide using a thermal plasma |
| CN102554242A (en) * | 2012-02-09 | 2012-07-11 | 西安宝德粉末冶金有限责任公司 | Method for manufacturing micro-fine spherical titanium powder |
| CN102910630A (en) * | 2012-10-15 | 2013-02-06 | 江苏博迁光伏材料有限公司 | Production method of nano silicon powder |
Non-Patent Citations (1)
| Title |
|---|
| 王耀军: "TIU-60感应等离子纳米粉末合成及应用", 《新技术新工艺》 * |
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Application publication date: 20160127 |